Process of manufacturing barium chlorid.



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E'INAR VAN'G GRANtjf OF LEONIA, -NEW JERSEY.

PROCESS OF, MANUFACTURING BAR-IUM CHLORIID.

No Drawing.

. T 0 all whom it may concern:

Be it known that I, EINAR VANG GRANo, a citizen of the United States,residing in Leonia, county of Bergen, andrState of New Jersey, haveinvented new and useful lmprovements in Processes of ManufacturingBarium Chlorid, of which the following is a specification.

This invention relates to the manufacture of barium chlorid from bariumsulfid ob-' sufficient quantities in the outlying localities where it isnecessary to set up plants for its production if the commercialmanufacture is to be successful.

I discovered that not only can a substanti ally quantitative yield ofbarium chlorid be obtained by the reaction of the chlorin gas (eitherobtained by electrolysis'or otherwise) upon a strong solution of bariumsulfid obtained by the reduction in the well known manner of baryteswith carbon and subsequent leaching of the furnaced product with Water,but that the employment of this method enables this process to becarried out in conjunction with other profitable processes whereinchlorin gas is obtained as a by-product. Moreover, in addition toobtaining a quantitative yield of barium chlorid, a substantiallyquantitative yield of sulfur in a finely precipitated condition can beobtained.

In carrying out my invention I preferably proceed as follows:Aconcentrated solution of barium chlorid is employed, preferably ofspecific gravity 20 B., the same being maintained at a temperature ofabout 85 C. The foregoing density'and tempera ture are desirable topreventcrystallization of barium hydroxid Ba(OI-l) suchsolutioncontaining approximately 178 grams of Bas per liter.Electrolytic chlorin gas is conducted into the solution, while the sameis maintained at the aforesaid temperature of approximately 85 C., andat a point a Specification of Letters Patent.

Patented Jan. 4, 1916.

Application filed'May 4, 1915. Serial No. 25,700.

sufficient distance from thebottom of the body of liquid to permittheprecipitated sulfur to settle to the bottom below the depth to which theagitating-effect of the gas 15 liable to exert itsinfluence or effectreaction. The object of this arrangement is to prevent the sulfurliberated by the chlorin gas from coming in contact with an excess ofchlorin whereby there would be a possibility of. the formation of smallquantities of sulfuric acid. Such acid would obviously instantaneouslydecompose a corresponding amount of BaS according to the followingreaction To prevent the sulfur already formed from being acted upon bythe chlorin gas in the aforesaid manner, a perforated false bottom isinserted in the precipitating vessel at a suitable depth below the lowerend of the pipe carrying the chlorin. The open ings in this false bottomare inch in diameter there belng 5 or' 6 to the square inch,

this being sufiicient to permit the sulfur to sink through to the bottomof the precipitating vessel. Preferably in a cylindrical tank 9 feethigh by 3 feet in diameter containing liquid to a height ofapproximately '8 feet, a pipe 1 inch in diameter projects into themiddle of the tank to a point 1% feet above the false bottom of saidtank, the said'false bottom being in turn placed 1 foot above the realbottom. By such arrange nent the agitating action. of-the gas will causeall sulfur as formed to pass through the perforated bottom after whichit will not be reacted upon by the free chlorin, since the same willpenetrate but little if at all below said bottom, the pressure underwhich the chlorin is introduced being adjusted to produce thedesiredagitatlon.

precipitated sulfur through the said false,

bottom. An exhaustive investigation of the aforesaid process showed thatIn order to determine to what extent this acid reaction This I (theoxidation of sulfur by chlorin to sul- I furic acid) will take placewhen the chlorin by being conducted into the bottom of the vessel isgiven every opportunity to react upon the nascent sulfur, shows thatthere will be as high as 12% of the total sulfur oxidized tosulfuricacid, whereas by my invention less than. 2% of sulfur was soconverted into sulfuric acid. During the first stages of the reaction itwill be observed that the sulfur liberated by the chlorin appears to bepartly dissolved by the remaining BaS, the-color of the solution being a'ohlorin ,While the sulfur is precipitated in ever increasing quantityso that when the process is finally completed the color of the liquidloses its yellow tint. almost instantaneously and becomes clear, whereasthe precipitated sulfur will then appear of a pale yellow or almostwhite color.

Having thus described my invention, What I claim and desire to secure byLetters Patent 1s':

1. The process which consists in subjecting a solution of barium sulfidto the action of chlorin gas. conducted into said solution from anexternal source, then permitting the same to react while constantlyremoving from the Zone of influence of said chlorin gas, the sulfurresulting from said reaction, a (1 then separately recovering the bariumc lorid and sulfur from said mixture.

2. In the process of making barium chlorid and sulfur the steps whichconsist in conducting chlorin gas into a concentrated solution ofbariumsulfid while maintaining the solution at a temperature sufficiently highto prevent crystallization of the barium hydroxid from said solution.

Signed at New York, countyand State of New York, this first 'day of May,1915.

EINAR VANG GRANO.

